纸基-表面增强拉曼光谱法快速鉴别染色南五味子药材

目的 采用纸基-表面增强拉曼光谱法(SERS)对染色南五味子进行快速鉴别。方法 选用浸泡法制备的银胶纸作为SERS基底,擦拭经乙醇-水溶液润湿的南五味子,银胶纸立即进行SERS检测;先后对银溶胶的浓缩倍数、银胶纸的SERS增强效果及稳定性等因素进行考察。结果 成功鉴别低浓度酸性红、赤藓红染色的南五味子。结论 纸基-SERS法可实现非法染色南五味子的快速、准确、无损的鉴别,有望应用于快检领域。     

Direct metabolic fingerprinting of olive oils using STELDI-MS

A new and rapid approach for analysis of olive oil has been developed using sorptive tape-like extraction in combination with laser desorption ionization mass spectrometry (STELDI-MS). This powerful combination has some great advantages, as no-separation steps, solvent-free, matrix-free, and no sample preparation. The olive oil compounds are analyzed by LDI-MS, directly from the sample spot in a thin-layer chromatography (TLC) plate. Chosen samples represent products commonly used as adulterants in extra virgin olive oil (EVOO) and the main monitored ions were lipid adulteration markers. Analytical procedures consisted of profiling the main fatty acids (m/z 255 – palmitic acid, 279 – linoleic acid, 281 – oleic acid and 283 – stearic acid), triacylglycerols (m/z 901 – LLL and 907 – OOO) and some phenolic compounds (m/z 169 – gallic acid, 193 – ferulic acid and 195 – 2(4-hydroxyphenyl) ethyl acetate) in extra virgin olive oil (EVOO), olive oil (OO), hazelnut oil (HO) and soybean oil (SO). Compound identification was confirmed by analysis of collision-induced dissociation (CID) products in positive (ion [M+Na]⁺) and negative mode (ion [M−H]⁻). This method is simple, fast and efficient in identifying compounds that can be used to recognize different levels of adulteration, oxidation and hydrolysis of vegetables oils.     

TLC-SERS联用法检测降糖中成药中添加的格列类药品

目的：研究降糖中成药中非法添加格列类药品的表面增强拉曼光谱（ surface enhanced Raman spectroscopy , SERS）检测方法。方法利用薄层色谱法将待检成分与中药基质进行简单分离,采用表面增强拉曼光谱技术对薄层板上的微量物质进行检测。通过摸索模拟阳性样品中格列类药品的SERS检测条件,建立可用于降糖中成药中非法添加物的检测方法。结果采用有机溶剂DMF制备所得的银溶胶可以获得较好的格列类药物SERS图谱。结论该研究所建立的TLC与SERS联用方法检测简便、快速、经济,可用于降糖中成药中非法添加格列类药品的快速检测。     

Hygienic quality,adulteration of pork and histamine production by Raoultella ornithinolytica in milkfish dumpling

Ten milkfish dumpling products purchased from retail stores in southern Taiwan were collected to determine the occurrence of biogenic amines, histamine-forming bacteria, and adulteration of pork. This study showed the high contents of aerobic plate count (APC), total coliforms (TC) and Escherichia coli in tested milkfish dumpling samples, whereas the average content of various biogenic amines in all tested samples was < 1.6 mg/100 g (< 0.05 to 1.54 mg/100 g). Three histamine-producing bacterial strains (2 isolates of Raoultella ornithinolytica and 1 isolate of Enterobacter aerogenes) isolated from tested samples produced 276.6 ppm to 561.8 ppm of histamine in trypticase soy broth supplemented with 1.0% L-histidine (TSBH). Assay of multiplex polymerase chain reaction (PCR) revealed that the adulteration rates were 50% (5/10) for pork in milkfish dumplings. In addition, milkfish dumpling stuffing was inoculated with R. ornithinolytica at 5.0 log colony forming units (CFU)/g and stored at various temperatures from 4°C to 37°C to investigate bacterial growth and formation of histamine. The histamine contents quickly increased to higher than 50 mg/100 g in samples stored at 37°C and 25°C within 24 hours and 36 hours, respectively, as well as stored at 15°C within 48 hours. Therefore, bacterial growth and histamine formation were controlled by cold storage of the samples at 4°C.     

Adulterants in selected dietary supplements and their detection methods

At present, there is a growing trend toward the intentional adulteration of dietary supplements (DS) with synthetic pharmaceuticals, which represents an alarming emerging risk to consumers and a serious problem for regulatory agencies. An amazing array of synthetic drugs and their analogues have been reported as adulterants in DS. Mainly, the presence of analogues represents a serious health risk as their efficacy and toxic effects have not been clinically assessed yet and may result in unpredictable adverse effects. The purpose of this review is to provide an overview, over the period 2009–2019, of the most frequently reported adulterants in DS for the treatment of erectile dysfunction, obesity/overweight, diabetes mellitus, and hypertension and the analytical methods used for their detection.     

Urinary melamine: Proposed parameter of melamine adulteration of food

Melamine is widely being reported as a food adulterant. Although its toxicity is currently recognized, melamine adulterations of food items are ongoing for falsely inflating the protein content of the food. Melamine alone or in combination with cyanuric acid or uric acid causes nephrotoxicity, and melamine-induced nephrotoxicity is now a global concern. It has been proven that when consumed, melamine is metabolized at a slower rate and excreted unchanged in urine. There is every possibility that when individuals consume melamine-adulterated food items, the melamine may be excreted unchanged in the urine. Therefore, melamine estimation in urine may be a yardstick to check for melamine adulteration of food items. In the present review, recent literature on this subject is analyzed justifying.     

Polyclonal antisera against unheated and heated common wheat specific gamma and omega gliadins for the detection of adulteration of durum wheat and durum wheat products with common wheats

Common wheat (Triticum aestivum L) specific gamma (y) and omega (a) gliadins from native (unheated) and heat‐processed (pasta) samples have been purified by reverse‐phase high‐pressure liquid chromatography and used to raise polyclonal antisera in New Zealand White rabbits. The sera have been examined in both the crude and affinity‐purified (against Durum flodur gliadins) states, for reactivity and specificity against gliadins from unheated and heat‐processed common wheats. Further, the antisera have been examined for cross‐reactivity against Durum wheat (Triticum durum Desf.) and pastas and for their potential as a means of detecting the adulteration of Durum wheats and Durum wheat pasta products with common wheat species (T. aestivum). The efficacy of the antisera was evaluated using two different immunoassay formats, enzyme‐linked immunosorbant assay (ELISA) and immunoblotting.     

丁香掺杂染色问题及检测方法研究

目的：4-甲基咪唑为焦糖色素制备过程中的一副产物,通过建立4-甲基咪唑的快速检测方法,控制丁香中花梗染焦糖色素后掺入样品。方法：采用高效液相色谱-质谱联用法,色谱柱为PhenomenexLuna C18（2 mm×150 mm,3μm）,以甲醇-0.1%甲酸溶液为流动相梯度洗脱,流速0.3 mL·min^-1,柱温30℃;质谱使用电喷雾离子源,正离子模式下检测。结果：4-甲基咪唑在9.28~371.11 ng·mL^-1浓度范围内呈良好的线性关系（r=0.9994）,平均回收率96.91%,RSD=1.0%;160批次丁香中33批次检出4-甲基咪唑,表明上述样品涉嫌染色。结论：本方法快速、简便、准确,专属性强,灵敏度高,可作为丁香中4-甲基咪唑的定性定量检测方法,为控制丁香质量提供参考。     

饮片茯苓掺伪的经验鉴别

目的杜绝掺伪茯苓,纯洁药品。方法采用性状鉴定+显微鉴定+理化鉴定的方法来辨别真假茯苓饮片。结果用上述联合鉴定的方法,能快速鉴别茯苓饮片是否掺伪。结论联合鉴别法能快速有效地鉴别茯苓饮片的真伪,简单易学。是基层用药单位鉴别茯苓饮片的一种有效的方法。同时提议茯苓饮片切制应尽量保持原生态,以利鉴别。     

减肥中成药中非法添加酚酞的拉曼光谱快速检测

目的:研究采用拉曼光谱法快速检测减肥中成药中非法添加的酚酞。方法:本文首先对4份减肥中成药样品各加入5 mL甲醇,超声10 min进行提取,接下来对提取液进行过滤,最后直接进行拉曼光谱的测试。结果:建立了酚酞-甲醇溶液的标准曲线,并且对添加不同质量浓度酚酞的减肥中成药进行拉曼光谱检测,所得结果与酚酞实际添加量一致。酚酞在0.1%以上浓度时,浓度与拉曼信号强度呈良好的线性关系(r=0.998 1),RSD 3.7%。结论:结合简单的前处理方法,拉曼光谱法可对减肥中成药中非法添加的酚酞进行快速筛查,并可进行定量分析;该方法快速、简便、成本低,检测限达1%,可同时得到定性与定量结果。